TW201446837A - Process pressure control in nylon synthesis - Google Patents

Abstract

A system is configured for continuous polyamide synthesis. The system includes a vent condenser and a vacuum pump. The vent condenser is coupled to a polymerization finisher. The vent condenser has a liquid reservoir and a vent discharge port above a level of the liquid reservoir. The vacuum pump is coupled to the vent discharge port by an intake line. The vacuum pump has an output port and a rotary shaft. A gaseous mixture proximate the vent discharge port is removed at a rate determined by a speed of the rotary shaft. The vacuum pump is configured to have a liquid ring seal.

Description

Process pressure control in nylon synthesis Cross-reference to related applications

The present application claims the priority of U.S. Provisional Patent Application Serial No. 61/818,240, filed on May 1, the entire entire entire entire entire entire content

Polyamines use diamines (such as hexamethylene-1,6-diamine) and dicarboxylic acids (such as adipic acid) (sometimes in the form of ammonium chloride in the form of two components in water) under polycondensation conditions. The process of polymerization (for example, at a temperature in the range of 180 ° C to 300 ° C) is produced. The condensation reaction produces polyamines (such as nylon 6,6) and water as by-products. In some cases, an early step in the process involves concentrating the ammonium formate brine solution, which is then passed to the reactor. The process of concentrating the ammonium formate brine will produce water which will be vented to the atmosphere as a vapor or condensed to form liquid water. The condensed liquid water is then typically discharged into the sewage system of the polyamine production facility.

The continuous polymerization manufacturing process can include a vented condenser downstream of the finishing machine. A gaseous mixture can be withdrawn from the vented condenser using a jet ejector. The jet injector creates a vacuum by flowing steam through a venturi device. A large amount of steam is passed through to draw a sufficient vacuum. In one example, about 450 Kg of steam per hour is required to create a sufficient vacuum. Steam production costs are high and the jet injector produces a substantial volume of waste steam. Additionally, the output of the jet injector may include contaminants drawn from the vent condenser. Contaminants may need to be removed, resulting in additional costs.

A problem with typical polymer synthesis processes is that they rely heavily on process steam. Process steam can be economically expensive in terms of production cost and can be environmentally expensive in terms of generating waste and consuming limited resources. In addition, it is not possible to control a process steam based system in a manner that produces a large volume of good quality product.

Examples of the subject matter of the present invention include a liquid ring vacuum pump. A liquid ring vacuum pump (LRVP) creates a vacuum by rotating blades in an eccentric chamber in the outer casing. The blade is fixedly coupled to the rotating shaft. The liquid ring around the eccentric chamber provides a seal with extremely low frictional resistance. The sealant ring is provided by water, oil or other fluid. In various examples, the sealing fluid is withdrawn from the vacuum or provided at the port on the pump housing. The LRVP can be a single or multi-stage pump.

An example of the subject matter of the present invention uses LRVP to control the manufacturing process. The LRVP can be used once through a sealed fluid supply or a recirculating sealed fluid supply or a blended sealed fluid supply. An example system using LRVP can operate economically and with good precision.

An example of the subject matter of the present invention uses LRVP to create a vacuum to extract a gaseous mixture from a vent condenser associated with the finishing machine in a continuous polymerization process.

In some examples, the subject LRVP of the present invention can provide a vacuum at substantially less energy consumption than the energy consumption associated with generating steam for use in a jet injector. In some instances, the LRVP of the present invention may be substantial in the polymer mixture during operation, as compared to methods of forming a vacuum in a polymer mixture using a device having a large amount of metal-to-metal contact, such as a mechanical impeller pump. Less impurities, such as less iron (which can be a gelling catalyst). In some instances, the amount of impurities (such as iron) generated during operation may be reduced to include LRVP as compared to a polymerization process including a mechanical impeller pump or other pump having greater metal to metal contact in the polymer mixture. The polymerization process experiences less gelation, providing high quality products and a greater percentage of start-up time.

This Summary of the Invention is intended to provide an overview of the subject matter of this patent application. Don't want to mention An exclusive or exhaustive explanation of the subject matter of the invention. [Embodiment] is included to provide additional information regarding this patent application.

8‧‧‧ pipeline

10‧‧‧System

12‧‧‧Reservoir

14‧‧‧Evaporator

16‧‧‧ pipeline

18‧‧‧Reactor

22‧‧‧ pipeline

24‧‧‧Condenser

26‧‧‧ pipeline

28‧‧‧ pipeline

30‧‧‧Flasher

32‧‧‧ pipeline

34‧‧‧ pipeline

200A‧‧‧ system

200B‧‧‧ system

208‧‧‧ Finishing machine

210‧‧‧Bend

212‧‧‧ Valve

214‧‧‧ arrow

216‧‧‧Ventilation condenser

218‧‧‧ dam

220‧‧‧ droplets

222‧‧‧ liquid level

224‧‧‧Reservoir

226‧‧‧ pipeline

228A‧‧‧ pipeline

228B‧‧‧ pipeline

228C‧‧‧ pipeline

230‧‧‧ liquid level

232‧‧‧ collection trough

234‧‧‧ dam

236‧‧‧ liquid level

238‧‧‧port

240‧‧‧ pipeline

242‧‧‧ arrow

246A‧‧‧Liquid ring vacuum pump

246B‧‧‧Liquid ring vacuum pump

246C‧‧‧Liquid ring vacuum pump

248A‧‧‧Axis

248B‧‧‧Axis

248C‧‧‧Axis

250A‧‧‧ electric motor

250B‧‧‧ electric motor

250C‧‧‧ electric motor

252A‧‧‧Filter

252B‧‧‧Filter

252C‧‧‧Filter

254‧‧‧ pipeline

256‧‧‧ arrow

258A‧‧‧ controller

258B‧‧‧ Controller

258C‧‧‧ Controller

260‧‧‧ processor

262‧‧‧ memory

264‧‧" interface

266‧‧‧ sensor

268‧‧‧ channel

270‧‧‧ computer

272‧‧‧ arrow

302‧‧‧ pump

304‧‧‧Filter

306‧‧‧cooler

308‧‧‧ Valve

310‧‧‧ valve

312‧‧‧ arrow

314‧‧‧ arrow

402‧‧‧ valve

404‧‧‧ pipeline

406‧‧‧ arrow

408‧‧‧ pipeline

412‧‧‧ arrow

414‧‧‧ Valve

416‧‧‧ Container

418‧‧‧ pipeline

420‧‧‧ pipeline

422‧‧‧ arrow

424‧‧‧ pipeline

426‧‧‧ pipeline

428‧‧‧ arrow

430‧‧‧ arrow

432‧‧‧ arrow

434‧‧‧ arrow

436‧‧‧ pipeline

438‧‧‧ arrow

In the drawings that are not necessarily drawn to scale, like numerals may depict similar components in different views. Similar numbers with different letter suffixes may indicate different execution individuals of similar components. The drawings generally illustrate, but are not limited to, the various examples discussed in the literature of the invention.

Figure 1 illustrates a schematic illustration of a system for making polyamines according to an example.

Figure 2 illustrates a portion of a polyamine production system in accordance with an example.

Figure 3 illustrates a portion of a polyamine production system in accordance with an example.

Figure 4 illustrates a portion of a polyamine production system in accordance with an example.

Figure 5 is a flow chart illustrating a method of making polyamine according to an example.

As used herein, the term "dicarboxylic acid" refers to a wide range C ₄ -C ₁₈ α, ω- dicarboxylic acid. This term encompasses C ₄ -C ₁₀ α,ω-dicarboxylic acid and C4-C8 α,ω-dicarboxylic acid. Examples of dicarboxylic acids encompassed by C ₄ -C ₁₈ α,ω-dicarboxylic acids include, but are not limited to, succinic acid/butanedioic acid, glutaric acid/pentanedioic acid, Adipic acid/hexanedioic acid, pimelic acid/heptanedioic acid, suberic acid/octanedioic acid, azelic acid/nonanedioic acid, and sebacic acid/ Decandedioic acid). In some embodiments, the C ₄ -C ₁₈ α,ω-dicarboxylic acid is adipic acid, pimelic acid or suberic acid. In some embodiments, the C ₄ -C ₁₈ α,ω-dicarboxylic acid is adipic acid.

As used herein, the term "diamine" refers to a wide range C ₄ -C ₁₈ α, ω- diamine. This term encompasses C ₄ -C ₁₀ α,ω-diamine and C ₄ -C ₈ α,ω-diamine. Examples of diamines encompassed by C ₄ -C ₁₈ α,ω-diamine include, but are not limited to, butane-1,4-diamine, penta-1,5-diamine, and hex-1,6-di An amine, also known as hexamethylenediamine. In some embodiments, the C ₄ -C ₁₈ α,ω-diamine is hexamethylenediamine.

In some examples, the use of adipic acid in combination with hexamethylene diamine is contemplated herein.

As used herein, the term "polyamine" broadly refers to polyamines such as nylon 6, nylon 7, nylon 11, nylon 12, nylon 6,6, nylon 6,9; nylon 6,10, nylon 6,12 or Copolymer.

In some examples, the polymer produced by performing the method or operating system is a polyamine. The polyamine can be synthesized from a linear dicarboxylic acid and a linear diamine or an oligomer formed from a linear dicarboxylic acid and a linear diamine. Polyamine can include nylon 6,6.

The dicarboxylic acid may have the structure HOC(O)-R ¹ -C(O)OH, wherein R ¹ is a C ₁ -C ₁₅ alkylene group such as methylene, ethyl, propyl, butyl, Stretching pentyl, stretching hexyl, stretching heptyl, stretching octyl, stretching sputum or stretching sputum. The dicarboxylic acid can be adipic acid (e.g., R ¹ = butyl).

The diamine may have the structure H ₂ NR ² —NH ₂ , wherein R ² is a C ₁ -C ₁₅ alkylene group, such as methylene, ethyl, propyl, butyl, pentyl, hexyl, Stretching the base, stretching the octyl group, stretching the base or stretching the base. The diamine can be adipic acid (e.g., R ² = butyl).

Figure 1 illustrates an example system 10 for producing polyamines and, in particular, nylon 6,6. System 10 includes various components that heat and vaporize water from a reaction mixture comprising oligomers formed from linear dicarboxylic acids and linear diamines. The oligomer formed from the linear dicarboxylic acid and the linear diamine may be a polyamine salt such as a hexanediamine adipate formed from a combination of adipic acid and hexamethylenediamine. The oligomer may comprise a combination of a single diacid molecule and a single diamine molecule, such as a hexanediamine adipate salt. An oligomer can be the product of one or more diacid molecules and one or more diamine molecules. Mixtures comprising oligomers may also include unreacted diamines and unreacted diacids. Mixtures comprising oligomers can include oligomers of various lengths in any suitable ratio.

Heating and evaporating a mixture comprising oligomers may be sufficient to remove at least some of the water from the mixture. In this document, when describing the removal of water, the removed water can be at least one of: water originally present in the mixture, produced by the reaction of a diacid with a diamine to form a guanamine. Raw water, water produced by the reaction of a diacid or a diamine with an oligomer to form a guanamine, and water produced by reacting an oligomer with another oligomer to form a guanamine.

System 10 can include a reservoir 12 configured to contain a solvent (e.g., water) in a liquid or substantially liquid phase and an aqueous solution of a mixture of a dicarboxylic acid and a diamine, and an oligomer (e.g., a salt formed thereby) ) or a combination thereof. The reservoir 12 can be used to mix or store an aqueous solution of ammonium formate.

Substantially equal molar ratios of dicarboxylic acid and diamine can be added to the reservoir 12. The starting material or aqueous solution may be preheated prior to introduction into the reservoir 12, such as with a preheater, or the aqueous solution may be in the reservoir 12 such as with a heater or with steam (such as steam formed in another portion of the system 10). ) Perform heating.

The reaction mixture can be passed from reservoir 12 to evaporator 14 via line 16. The evaporator 14 can heat the reaction mixture and thereby evaporate the water, thereby pushing the equilibrium further toward the polyamide product. Water evaporated from the reaction mixture in evaporator 14 can exit evaporator 14 via line 8. The reaction mixture can be heated in evaporator 14 to any suitable temperature, such as about 100-230 ° C, or 100-150 ° C, or about 100 ° C or less, or about 110 ° C, 120 ° C, 130 ° C, 140 ° C. , 150 ° C, 160 ° C, 170 ° C, 180 ° C, 190 ° C, 200 ° C, 210 ° C, 220 ° C or about 230 ° C or more. The reaction mixture exiting evaporator 14 via line 22 can have any suitable weight percentage of water, such as from about 5 to 50 weight percent water, or from about 25 to 35 weight percent water, or from about 25 weight percent or less to 26 weight percent, 26 weight percent. %, 27% by weight, 28% by weight, 29% by weight, 30% by weight, 31% by weight, 32% by weight, 33% by weight, 34% by weight or about 35% by weight or more by weight of water. The reaction mixture in evaporator 14 can be passed to reactor 18 via line 22.

Reactor 18 can heat the reaction mixture and thereby evaporate water, thereby pushing the equilibrium further toward the polyamide product. Water evaporating from the reaction mixture in reactor 18 can exit via line 26 and enter condenser 24 where it can condense to form liquid water exiting condenser 24 with line 28. The liquid water in line 28 can be suitably in other components of the facility It is treated and reused in the reservoir 12 or may be placed in a sewer. The heat absorbed by the condenser 24 can be reused in other components of the facility, such as in a preheater. The reaction mixture can be heated in reactor 18 to any suitable temperature, such as from about 150 to 400 ° C, or from about 250 to 350 ° C, or from about 250 to 310 ° C, or from about 200 ° C or below, or from about 210 ° C, 220. °C, 230°C, 240°C, 250°C, 260°C, 265°C, 270°C, 275°C, 280°C, 285°C, 290°C, 295°C, 300°C, 305°C, 310°C, 320°C, 330°C, 340 ° C or about 350 ° C or above. The reaction mixture exiting reactor 18 via line 32 can have any suitable weight percentage of water, such as from about 0.0001% to 20% by weight, from 0.001% to 15% by weight, or from about 0.01% to 15% by weight, or from about 0.0001% % by weight or 0.0001% by weight or less, or about 0.001% by weight, 0.01% by weight, 0.05% by weight, 0.06% by weight, 0.07% by weight, 0.08% by weight, 0.09% by weight, 0.1% by weight, 0.2% by weight, 0.3% by weight, 0.4% by weight, 0.5% by weight, 0.6% by weight, 0.7% by weight, 0.8% by weight, 0.9% by weight, 1.0% by weight, 1.2% by weight, 1.4% by weight, 1.6% by weight, 1.8% by weight, 2% by weight, 3 parts by weight %, 4% by weight, 5% by weight, 6% by weight, 7% by weight, 8% by weight, 9% by weight, 10% by weight, 11% by weight, 12% by weight, 13% by weight, 14% by weight, 15% by weight, 16% by weight, 17% by weight, 18% by weight, 19% by weight or about 20% by weight or more. The reaction mixture in reactor 18 can be passed via line 32 to flasher 30.

The flasher 30 can heat the reaction mixture and thereby evaporate the water, thereby pushing the equilibrium further toward the polyamide product. Flasher 30 can include at least one relatively long serpentine tube. Within the flasher 30, the pressure may gradually decrease as the reaction mixture travels downstream. At elevated temperatures within the flasher 30, the decreasing pressure applied to the reaction mixture removes water from the reaction mixture as flash vapor. When steam is flashed from the reaction mixture, the first polyamide polymer can undergo further polymerization to form a second polyamide polymer. At the exit of flasher 30, a two phase mixture of gaseous vapor and reaction mixture can be formed. The reaction mixture can be heated in flasher 30 to any suitable temperature, such as about 150-400 ° C, or about 250-350 °C, or about 250-310 ° C, or about 200 ° C or below, or about 210 ° C, 220 ° C, 230 ° C, 240 ° C, 250 ° C, 260 ° C, 265 ° C, 270 ° C, 275 ° C, 280 ° C, 285 ° C, 290 ° C, 295 ° C, 300 ° C, 305 ° C, 310 ° C, 320 ° C, 330 ° C, 340 ° C or about 350 ° C or above. The reaction mixture exiting flasher 30 via line 34 can have any suitable weight percentage of water, such as from about 0.0001 wt% to 2 wt%, from 0.001 wt% to 1 wt%, or from about 0.01 wt% to 1 wt%, or from about 0.0001. % by weight or 0.0001% by weight or less, or about 0.001% by weight, 0.01% by weight, 0.05% by weight, 0.1% by weight, 0.2% by weight, 0.3% by weight, 0.4% by weight, 0.5% by weight, 0.6% by weight, 0.7% by weight, 0.8% by weight, 0.9% by weight, 1.0% by weight, 1.2% by weight, 1.4% by weight, 1.6% by weight, 1.8% by weight or about 2% by weight or more. The reaction mixture in flasher 30 can be passed to line 208 via line 34.

Finisher 208 can heat the reaction mixture and thereby evaporate the water, thereby pushing the equilibrium further toward the polyamine product, such that a polyamine product of the final desired degree of polymerization is obtained. The finisher 208 can remove additional water such that the second polyamide polymer undergoes further polymerization to form a final polyamine polymer having a final desired molecular weight or a desired molecular weight range. The final desired molecular weight or desired molecular weight range may depend on the final specific desired characteristics of the polyamine product. Removal of water in the finisher 208 can be accomplished by applying high temperature and vacuum pressure to the reaction mixture. The final molecular weight range of the final polyamide polymer can be controlled by controlling the vacuum pressure applied to the finisher 208 and the residence time of the reaction mixture within the finisher 208. The reaction mixture can be heated in the finishing machine 208 to any suitable temperature, such as about 150-400 ° C, or about 250-350 ° C, or about 250-310 ° C, or about 200 ° C or below, or about 210 ° C, 220°C, 230°C, 240°C, 250°C, 260°C, 265°C, 270°C, 275°C, 280°C, 285°C, 290°C, 295°C, 300°C, 305°C, 310°C, 320°C, 330°C , 340 ° C or about 350 ° C or above. The reaction mixture exiting the finisher 208 can have any suitable weight percentage of water, such as from about 0.0001% to 2% by weight, from 0.001% to 1% by weight, or from about 0.01% to 1% by weight, or from about 0.0001% by weight. or 0.0001% by weight or less, or about 0.001% by weight, 0.01% by weight, 0.05% by weight, 0.1% by weight, 0.2% by weight, 0.3% by weight, 0.4% by weight, 0.5% by weight, 0.6% by weight, 0.7% by weight, 0.8% by weight 0.9% by weight, 1.0% by weight, 1.2% by weight, 1.4% by weight, 1.6% by weight, 1.8% by weight or about 2% by weight or more.

Emissions from finishing machine 208 are routed downstream for further processing. Further processing can include adjusting relative viscosity, centrifugal rotation, and granulation. The reaction mixture in finishing machine 208 comprises a polyamidamine having a desired degree of polymerization, and in one example, at a temperature of about 280 °C.

In the manufacture of nylon 6,6, cross-linking of polyamine is undesirable because it causes gel formation in the polyamide synthesis process. Gel formation in turn leads to polyamine contamination that requires more frequent equipment maintenance and associated equipment downtime.

The examples of the subject matter of the present invention are directed to controlling the relative viscosity of the products of the synthetic process. Relative viscosity is a measure of the ratio of solution to solvent viscosity as measured by capillary viscosity at a particular temperature. According to ASTM D789-06, the relative viscosity is the viscosity (in centipoise) of 8.4% by weight of polyamine in 90% formic acid (90% by weight formic acid and 10% by weight of water) at 25 ° C and 25 ° C alone The ratio of the viscosity of 90% formic acid (in centipoise). The relative viscosity can be related to the measure of molecular weight.

In one example, the relative viscosity is adjusted by drawing a controlled vacuum to the vent condenser using a liquid ring vacuum pump. The discharge condenser is coupled to a polymerization finisher 208. Adjusting the relative viscosity can include implementing a feedback process using a sensor and controller coupled to the motor drive of the LRVP.

2 illustrates a system 200A that depicts one processing example associated with finishing machine 208 and certain components downstream of finishing machine 208.

Material from the finishing machine 208 is conveyed to the vent condenser 216 using a bend 210. The material flows in the direction indicated by arrow 272.

In the illustrated example, the vent condenser 216 includes a dam having an upper region disposed therein 218 vertical column. Barrage 218 may include an annular wall having an open top and a closed bottom. Water (or other fluid) delivered to the barrage 218 may overflow from the top, and in this example, appear as a drop 220 that falls into the reservoir 224 at the bottom of the vent condenser 216. Water is supplied to the barrage 218 by valve 212 as indicated by arrow 214.

In addition to or instead of the barrage 218, the vent condenser 216 can include a spray nozzle. A spray nozzle (not shown in the illustrated example) can dispense water flow, water droplets or atomized water in the upper region of the vent condenser 216.

Returning the flow rate of the vent condenser 216 can affect the turbulence in the vent condenser 216. For example, at high flow rates (at valve 212), spatter can create more aerosol in the gaseous mixture above reservoir 224, and thus affect downstream equipment. Water flow rate, nozzle configuration, dam configuration 218, vacuum and other factors can be selected to achieve the desired production parameters. The water in the reservoir 224 has a liquid level 222.

The effluent from the reservoir 224 is delivered to the collection tank 232 by line 228A (sometimes referred to as a pneumatic line). Collection trough 232 (sometimes referred to as a hot well) includes a barrage 234. Barrage 234 retains material in collection trough 232 until the volume exceeds liquid level 230 (established by the height of barrage 234). Water at level 236 is discharged from collection tank 232 via line 240 via port 238 as indicated by arrow 242. Line 240 can be coupled to a sump (not shown) or a sewer system (not shown).

The gaseous material in the vent condenser 216 is carried by vacuum in line 226. Line 226 is coupled to vent condenser 216 at a location above liquid level 222.

Liquid ring vacuum pump 246A draws a vacuum in line 226 and discharges the output to filter 252A. Filter 252A can include a stacked scrubber. In the illustrated example, the effluent from filter 252A is vented to the atmosphere by line 254 in the direction indicated by arrow 256.

In one example, the amount of vacuum drawn by the liquid ring vacuum pump 246A is determined by the rotational speed of the shaft 248A. Shaft 248A is coupled to motor 250A in this example. Motor 250A is powered by a metered pipeline facility (not shown) and is controlled by controller 258A. In an instance The motor 250A has a power rating of approximately three horsepower. In one example, motor 250A is non-electric and provides other means of controlling shaft speed.

In the illustrated example, controller 258A includes a computer 270 coupled to sensor 266. The computer 270 includes a processor 260, a memory 262, and an interface 264. Memory 262, interface 264, and sensor 266 are in communication with processor 260. Processor 260 is configured to execute instructions to implement an algorithm to control LRVP 246A. The algorithm may include operating the motor 250A based on signals from the sensor 266. The memory 262 stores instructions and data related to controlling the LRVP 246A. Interface 264 may include a keyboard, trackpad, screen, printer, network interface, or other components configured to allow a user to monitor or control the performance of LRVP 246A.

The sensor 266 is coupled to 270 via a channel 268. Channel 268 can include a wired or wireless communication link. The sensor 266 can include a pressure sensor, a vacuum sensor, a flow sensor, a temperature sensor, a level sensor, a clock, a load sensor, or configured to provide controllable operation of the LRVP 246A. The other components of the signal.

Alternatively, the amount of vacuum drawn can be controlled by adjusting the valve associated with the LRVP 246A. For example, the valve can be configured to bypass LRVP 246A or configured to ventilate the low (vacuum) side or high (pressure) side of LRVP 246A. The valve position can be controlled by the processor 260 based on signals from the sensor 266.

The LRVP 246A extracts any suitable volume of gas from the finishing machine. In some examples, the liquid ring vacuum pump can draw from about 10 m ³ /h to about 50,000 m ³ /h, from about 20 m ³ /h to about ^30,000 m ³ /h, from about 50 m ³ /h to about 20,000 m ³ /h, or About 10 m ³ /h or 10 m ³ /h or less, or about 20 m ³ /h, 30 m ³ /h, 40 m ³ /h, 50 m ³ /h, 75 m ³ /h, 100 m ³ /h, 125 m ³ /h, 150 m ³ /h, 175m ³ /h, 200m ³ /h, 250m ³ /h, 300m ³ /h, 400m ³ /h, 500m ³ /h, 600m ³ /h, 700m ³ /h, 800m ³ /h, 900m ^{3 / h, 1,000m 3 / h} , 1,500m 3 / h, 2,000m 3 / h, 2,500m 3 / h, 5,000m 3 / h, 10,000m 3 / h, 20,000m 3 / h, 30,000m 3 / h, 40,000 m ³ /h or about 50,000 m ³ /h.

LRVP 246A can be made from any suitable material or combination of materials. In some examples, LRVP 246A can include any suitable proportion of stainless steel, such as austenitic steel, ferromagnetic steel, martensitic steel, and combinations thereof. The stainless steel may comprise any suitable series of stainless steels, such as 440A, 440B, 440C, 440F, 430, 316, 409, 410, 301, 301LN, 304L, 304LN, 304, 304H, 305, 312, 321, 321H, 316L, 316, 316LN, 316Ti, 316LN, 317L, 2304, 2205, 904L, 1925hMo/6MO, 254SMO. The austenitic steel may comprise 300 series steel, for example having up to about 0.15% carbon, at least about 16% chromium, and sufficient nickel or manganese to maintain the austenitic structure at substantially all temperatures from the low temperature region to the melting point of the alloy. Austenitic steels may include, for example, 304 and 316 steels, such as 316L steel. In some examples, LRVP 246A can include a corrosion resistant material. Examples of corrosion resistant materials may include superalloys such as nickel-copper alloy containing a small amount of iron and trace amounts of other elements, such as MONEL ^® 400; precipitation hardening nickel-iron-chromium alloy, such as INCOLOY ^® brand alloy, such as INCOLOY ^® 800 series; or Austria 's body nickel chromium matrix card INCONEL ^® alloy, or a nickel-chromium-molybdenum alloy, such as HASTELLOY ^® brand alloy, such as HASTELLOY ^® G-30 ^®. Examples of corrosion resistant materials may include any suitable corrosion resistant material, such as super austenitic stainless steel (eg, AL6XN, 254SMO, 904L), duplex stainless steel (eg, 2205), super duplex stainless steel (eg, 2507), nickel based alloy (eg, Alloys C276, C22, C2000, 600, 625, 800, 825), titanium alloys (eg grade 1, grade 2, grade 3), zirconium alloys (eg 702), Hasteloy 276, duplex 2205, super duplex 2507, Ebrite 26-1, Ebrite 16-1, Hasteloy 276, duplex 2205, 316 SS, 316L and 304SS, zirconium, zirconium composite 316, iron 255 or any combination thereof.

LRVP 246A reduces the costs associated with jet injectors, such as the cost of water and the cost of generating steam. The LRVP 246A provides significant energy cost savings compared to jet injectors, despite the electrical cost of the motor 250A. For example, LRVP 246A may provide an energy cost of from 0.01% to 95% of the energy cost of the steam injector, or from about 1% to about 80%, or about 0.01% or less, of the energy cost of the steam injector, About 0.1%, 1%, 2%, 4%, 6%, 8%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90% or about 95%.

The LRVP 246A can be configured to have less metal to metal contact in the polymer mixture than other devices such as mechanical impeller pumps. For example, by using a liquid ring as a seal, the LRVP 246A avoids metal and metal wear between the impeller tips and within the pump casing. In some examples, LRVP 246A can have from about 0.0001 ppm to about 200 ppm iron, or from about 0.001 ppm to about 25 ppm iron, or from about 0.0001 ppm or 0.0001 ppm, 0.0005 ppm, 0.001 ppm, in the polymer reaction mixture exiting the pump. 0.005 ppm, 0.01 ppm, 0.05 ppm, 0.1 ppm, 0.5 ppm, 1 ppm, 1.5 ppm, 2 ppm, 2.5 ppm, 3 ppm, 4 ppm, 5 ppm, 6 ppm, 7 ppm, 8 ppm, 9 ppm, 10 ppm, 15 ppm, 20 ppm, 25 ppm, 30 ppm, 35 ppm 40 ppm, 45 ppm, 50 ppm, 75 ppm, 100 ppm, 125 ppm, 150 ppm, 175 ppm or about 200 ppm or more. The parts per million of iron in the reaction mixture leaving the pump can be any suitable amount less than parts per million of iron in the corresponding reaction mixture exiting the mechanical impeller pump, such as from about 0.01% to 95%, or from about 1% to about 80. %, or about 0.01% or less, about 0.1%, 1%, 2%, 4%, 6%, 8%, 10%, 15%, 20%, 25%, 30%, 35%, 40% 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90% or about 95%. Iron can be a gel catalyst; reducing iron content can reduce gel production. The gel produced daily downstream of the pump can be any suitable amount and can be substantially proportional to the reduction in iron content of the reaction mixture drawn from the pump, less than the amount produced by the corresponding reaction mixture exiting the mechanical impeller pump, such as about daily. 0.0001Kg gel to about 100Kg gel per day, about 0.001Kg gel per day to about 50Kg gel per day, or about 0.0001Kg gel per day, 0.0005Kg, 0.001Kg, 0.005Kg, 0.01Kg, 0.05Kg, 0.1Kg per day 0.5 Kg, 1 Kg, 2 Kg, 3 Kg, 4 Kg, 5 Kg, 10 Kg, 15 Kg, 20 Kg, 25 Kg, 50 Kg, 75 Kg or about 100 Kg gel.

3 illustrates a system 200B that depicts certain downstream of finishing machine 208 and finishing machine 208. A processing example related to components.

Material from the finishing machine 208 is conveyed to the vent condenser 216 using a bend 210. The material flows in the direction indicated by arrow 272.

In the illustrated example, the vent condenser 216 includes a vertical column having a dam 218 disposed in the upper region. Barrage 218 may include an annular wall having an open top and a closed bottom. Water (or other fluid) delivered to the barrage 218 may overflow from the top, and in this example, appear as a drop 220 that falls into the reservoir 224 at the bottom of the vent condenser 216. Water is supplied to the barrage 218 by valve 308 as indicated by arrow 314.

The water in the reservoir 224 has a liquid level 222. Line 228B brings water from reservoir 224 to pump 302.

Pump 302 carries the effluent from reservoir 224 to filter 304. Pump 302 is drawn from line 228B coupled to reservoir 224. Valve 310 causes excess water to be discharged as indicated by arrow 312. The water discharged from the valve 310 can be discharged into a tank (not shown) or a sewer system (not shown). Valve 310 can be automatically adjusted to control the level of water that is recirculated by pump 302. Filter 304 is in series with cooler 306 and valve 308.

The gaseous material in the vent condenser 216 is carried by the vacuum in line 226. Line 226 is coupled to vent condenser 216 at a location above liquid level 222.

Liquid ring vacuum pump 246B draws a vacuum in line 226 and discharges the output into filter 252B. Filter 252B can include a stacked scrubber. In the illustrated example, the effluent from filter 252B is vented to the atmosphere by line 254 in the direction indicated by arrow 256.

The amount of vacuum drawn by the liquid ring vacuum pump 246B is determined by the rotational speed of the shaft 248B. Shaft 248B is coupled to motor 250B in this example. Motor 250B is powered by a metered pipeline facility (not shown) and is controlled by controller 258B.

Controller 258B can include an analog processor or a digital processor. In one example, controller 258B includes processor 260, memory 262, interface 264, and sensor 266.

4 illustrates a system 200C that depicts certain downstream of finishing machine 208 and finishing machine 208. A processing example related to components.

Material from the finishing machine 208 is conveyed to the vent condenser 216 using a bend 210. The material flows in the direction indicated by arrow 272.

In the illustrated example, the vent condenser 216 includes a vertical column having a dam 218 disposed in the upper region. Barrage 218 may include an annular wall having an open top and a closed bottom. Water (or other fluid) delivered to the barrage 218 may overflow from the top, and in this example, appear as a drop 220 that falls into the reservoir 224 at the bottom of the vent condenser 216.

In one example, water is supplied to the barrage 218 by line 408, valve 402, and line 404 as indicated by arrows 412 and 406. As indicated by arrow 412, the water supply can include demineralized water.

The water in the reservoir 224 has a liquid level 222. Emissions from reservoir 224 are discharged using line 228C as indicated by arrow 428.

The gaseous material in the vent condenser 216 is carried by the vacuum in line 420 as indicated by arrow 430. The first end of the line 420 is coupled to the vent condenser 216 (at a position above the liquid level 222) and the second end is coupled to the vessel 416. Container 416 can be considered a vapor-liquid separator.

The vessel 416, sometimes referred to as a separation weir, has a discharge port coupled to the vacuum line 418. Line 418 carries a gaseous mixture from vessel 416 (as indicated by arrow 432), and thus, vent condenser 216 is evacuated via line 420. Process steam is condensed in vessel 416 and the resulting water is withdrawn through line 426 and taken away as indicated by arrow 428. Water is supplied to vessel 416 by line 408 as indicated by arrow 434.

Liquid ring vacuum pump 246C draws a vacuum in line 418 and discharges the output to filter 252C. Filter 252C can include a stacked scrubber. In the illustrated example, the effluent from filter 252C is vented to the atmosphere by line 254 in the direction indicated by arrow 256. Water is drained from filter 252C by line 424 in the direction indicated by arrow 422.

The sealing fluid of LRVP 246C is supplied by line 436 in the direction indicated by arrow 438. In one example, the sealing fluid includes water, and thus line 436 can be coupled to the pipeline 408 or another supply line. In the example shown in Figures 2 and 3, the sealing fluids of LRVP 246A and LRVP 246B are supplied by vent condenser 216, respectively, however, in other examples (such as shown in LRVP 246C in Figure 4), A supply line (e.g., line 436) provides a sealed fluid to vacuum pump 246C.

The first end of the valve 414 is coupled to the line 418 and the second end is coupled to the discharge port from the line 254. Valve 414 can be adjusted to bypass LRVP 246C and thus control the vacuum drawn by vessel 416.

The amount of vacuum drawn by the LRVP 246C is determined by the rotational speed of the shaft 248C. Shaft 248C is coupled to motor 250C in this example. Motor 250C is powered by a metered pipeline facility (not shown) and is controlled by controller 258C.

Controller 258C can include an analog processor or a digital processor. In one example, controller 258C includes processor 260, memory 262, interface 264, and sensor 266.

Figure 5 illustrates a flow diagram of a method 500 of making polyamine. The method 500 includes, at 510, creating a gaseous mixture over the reservoir 224. The reservoir 224 in the continuous polyamine synthesis system can include condensation with a vent condenser 216 coupled to the polymerization finisher 208.

At 520, method 500 includes withdrawing the gaseous mixture using a vacuum pump 246C. Vacuum pump 246C may include LRVP 246C driven by motor 250C. The degree of vacuum can be determined based on the speed of the rotating shaft 248C of the LRVP 246C and thereby the rate of removal of the gaseous mixture can be determined.

The drive motor 250C of the LRVP 246C can be controlled or adjusted using the controller 258C. Controller 258C can include an analog circuit or a digital processor. In the case of a digital processor, the LRVP 246C can be controlled by implementing software in the memory 262 that is programmed to store instructions. In various examples, the algorithm uses sensor signals to control the LRVP 258C. The sensor signal can be generated by a sensor 266 that is responsive to pressure, vacuum, temperature, level, load, or other measurement parameters.

The LRVP 246C utilizes a fluid ring to provide a seal. The sealing fluid can be supplied by condensate in vacuum line 418 or by separate fluid ports. Sealing fluid can include water, oil Or other fluids. The fluid supplied to the liquid ring of LRVP 246C is heated by the action of rotating blades, and in one example, the fluid is recovered, filtered, cooled, and recycled to LRVP 246C at a flow rate of about 1 to 5 gallons per minute. In one example, a continuous polymerization process uses fresh water for sealing fluid. In one example, the batch polymerization process will be used to seal the fluid in the future.

Instance

Continuous polymerization process. Perform the following process in the examples given in this section. In a continuous nylon 6,6 manufacturing process, adipic acid and hexamethylenediamine are combined in water in about a molar ratio to a salt trigger to form an aqueous mixture containing a nylon 6,6 salt having about 50% by weight water. The brine solution was passed to the evaporator at about 105 L/min. The evaporator heats the brine solution to about 125-135 ° C (130 ° C) and removes the water from the heated brine solution to a water concentration of about 30% by weight. The evaporated salt mixture was passed to the reactor at about 75 L/min. The reactor raises the temperature of the evaporated salt mixture to about 218-250 ° C (235 ° C), allowing the reactor to further remove water from the heated evaporated salt mixture to a water concentration of about 10% by weight and further salt polymerization. The reaction mixture was passed to the flasher at about 60 L/min. The flasher heats the reaction mixture to about 270-290 ° C (280 ° C), allowing the flasher to further remove water from the reaction mixture, thereby bringing the water concentration to about 0.5% by weight, and further polymerizing the reaction mixture. The flashed mixture was transferred to the finisher at about 54 L/min. The finishing machine subjects the polymerization mixture to a vacuum to further remove water such that the water concentration reaches about 0.1% by weight such that the polyamide reaches a suitable final degree of polymerization, after which the finished polymerization mixture is transferred to the extruder and pellets. Chemical machine.

A general method for determining the gelation rate. The gelation rates described in the examples were determined by taking the average of the gelation rates as determined by the two methods. In the first method, when the reaction mixture is still hot, the system is allowed to drain the liquid reaction mixture, the system is cooled, disassembled, and visually inspected to estimate the volume of the gel therein. In the second method, when the reaction mixture is still hot, the system is allowed to drain the liquid reaction mixture, cooled, filled with water and drained. The volume of gel in the system is determined by subtracting the volume of water discharged from the system from the gel-free volume of the system. To determine the gelation rate in one or more specific equipment or downstream of a specific location, only the downstream of the particular equipment or system specific location is filled with water. In both methods, the density of the gel was estimated to be 0.9 g/cm ³ .

The variable X has the same value throughout the instance.

Example 1a. Comparative example. Finishing machine with pneumatic vacuum column recirculation and mechanical impeller pump.

Perform a continuous aggregation process. The effluent from the finishing machine is delivered to a vent condenser. The vent condenser includes a liquid reservoir containing a discharge line. A discharge line, sometimes referred to as a pneumatic vacuum column, is coupled to the low point of the reservoir. A pump coupled to the pneumatic vacuum column delivers liquid from the reservoir to the filter and cooler, and thereafter returns the fluid to the dam and sprayer configuration located above the vent condenser.

The vacuum line is coupled to the point of the vent condenser that is above the liquid reservoir. The vacuum line is coupled to a 304 austenitic steel mechanical impeller pump that draws 1000 m ³ /h. The vacuum pump is discharged into the scrubber and thereafter vented to the atmosphere. The power supplied by the mechanical impeller pump costs about X per year. The polymer mixture exiting the mechanical impeller pump has about 3 ppm iron. The total amount of gel produced downstream of the vacuum pump in the system is about 0.5 Kg gel per day.

Example 1b. Comparative example. Finishing machine with pneumatic vacuum column recirculation and steam injector.

According to Comparative Example 1, but instead of a mechanical impeller pump, a 304 austenitic steel vapor injector was used which extracted 1000 m ³ /h. The steam ejector uses 34,000,000 Kg of steam per year and costs 3 x X per year. Steam requires 1,500,000,000 L of water per year and costs X per year. Therefore, the steam ejector requires about 4 x X to operate each year.

Example 1c: Finishing machine with pneumatic vacuum column recirculation and liquid ring vacuum pump.

Perform a continuous aggregation process. The effluent from the finishing machine 208 is delivered to a vent condenser 216. The vent condenser 216 includes a liquid reservoir 224 that is equipped with a discharge line. A discharge line, sometimes referred to as a pneumatic vacuum column, is coupled to the low point of the reservoir 224. A pump coupled to the pneumatic vacuum column delivers liquid from the reservoir 224 to the filter and cooler 306, and thereafter flows The body returns to the barrage 218 and the sprayer configuration located above the vent condenser 216.

Vacuum line 420 is coupled to a point above vent condenser 216 that is above liquid reservoir 224. The vacuum line 420 is coupled to a 304 austenitic steel liquid ring vacuum pump 246C which draws 1000 m ³ /h. The LRVP 246C is vented to the scrubber and thereafter vented to the atmosphere. The polymer mixture leaving LRVP 246C contained about 0.5 ppm iron, which reduced the total amount of gel produced downstream of the vacuum pump in the system to about 0.1 Kg gel per day, which was the gel production in the process of Comparative Example 1a including the mechanical impeller pump. 20% of the rate results in longer start-up times between shutdowns and cleaning. The power supplied to the LRVP 246C via the drive motor 250C is approximately X per year, such that the process is about 400% more efficient than the process including the steam injector in Comparative Example 1b.

Example 2a: Comparative example. Finishing machine with pneumatic vacuum column discharge and mechanical impeller pump.

Perform a continuous aggregation process. The effluent from the finishing machine is delivered to a vent condenser. The vent condenser includes a liquid reservoir containing a discharge line. A discharge line, sometimes referred to as a pneumatic vacuum column, is coupled to the low point of the reservoir. The liquid in the pneumatic vacuum column is sent to the collection tank as a path. Collection tanks, sometimes referred to as hot wells, include dams and vents. The collection tank is discharged into the sewage pipe. The respective water supply lines are coupled to a dam and sprayer configuration located above the vent condenser.

The vacuum line is coupled to the point of the vent condenser that is above the liquid reservoir. The vacuum line is coupled to a 304 austenitic steel mechanical impeller pump that draws 1000 m ³ /h. The vacuum pump is discharged into the scrubber and thereafter vented to the atmosphere. The power supplied by the mechanical impeller pump costs about X per year. The polymer mixture exiting the mechanical impeller pump has about 3 ppm iron. The total amount of gel produced downstream of the vacuum pump in the system is about 0.5 Kg gel per day.

Example 2b: Comparative example. Finishing machine with air pressure vacuum column discharge and steam injector.

According to Comparative Example 2, but instead of a mechanical impeller pump, a 304 austenitic steel vapor injector was used which extracted 1000 m ³ /h. The steam ejector uses 34,000,000 Kg of steam per year and costs 3 x X per year. Steam requires 1,500,000,000 L of water per year and costs X per year. Therefore, the steam ejector requires about 4 x X to operate each year.

Example 2c: Finishing machine with air pressure vacuum column discharge and liquid ring vacuum pump.

Perform a continuous aggregation process. The effluent from the finishing machine 208 is delivered to a vent condenser 216. The vent condenser 216 includes a body reservoir 224 that is filled with a discharge line. A discharge line, sometimes referred to as a pneumatic vacuum column, is coupled to the low point of the reservoir 224. The liquid in the pneumatic vacuum column is sent to the collection tank 232 in a path. A collection tank 232, sometimes referred to as a hot well, includes a dam 234 and a vent. The collection tank 232 is discharged into the sewage pipe. The respective water supply lines are coupled to a dam 218 and a sprayer configuration located above the vent condenser 216.

Vacuum line 226 is coupled to the point of vent condenser 216 above the liquid reservoir. Vacuum line 226 is coupled to 304 austenitic steel LRVP 246A which draws 1000 m ³ /h. The LRVP 246A is vented to the scrubber and thereafter vented to the atmosphere. The polymer mixture exiting LRVP 246A contained about 0.5 ppm iron, which reduced the total amount of gel produced downstream of the vacuum pump in the system to about 0.1 Kg per day, which is the rate of gel production in the process including the mechanical impeller pump in Comparative Example 2a. 20%, resulting in a long start-up time between shutdowns and cleaning. The power supplied to the liquid ring vacuum pump via the drive motor 250A was spent X per year, so that the process was about 400% more efficient than the process including the steam injector in Comparative Example 2b.

Example 3a: Comparative example. Finishing machine with vapor-liquid separator and mechanical impeller pump.

Perform a continuous aggregation process. The effluent from the finishing machine is delivered to a vent condenser. The vent condenser includes a liquid reservoir containing a discharge line. A discharge line, sometimes referred to as a pneumatic vacuum column, is coupled to the low point of the reservoir.

The vacuum line is coupled to the point of the vent condenser that is above the liquid reservoir. The vacuum line is coupled to the input of the vapor-liquid separator. The liquid withdrawn from the low point of the vapor-liquid separator is routed to the coupling on the pneumatic vacuum column. The gaseous mixture above the liquid in the vapor-liquid separator was withdrawn via a vacuum line coupled to a 304 austenitic steel mechanical impeller pump which withdrawn 1000 m ³ /h. The vacuum pump is discharged into the scrubber and thereafter vented to the atmosphere. The power supplied by the mechanical impeller pump costs about X per year. The polymer mixture exiting the mechanical impeller pump has about 3 ppm iron. The total amount of gel produced downstream of the vacuum pump in the system is about 0.5 Kg gel per day.

The respective water supply lines are coupled to the dam and sprayer configuration above the vent condenser and above the vapor-liquid separator.

Example 3b: Comparative example. With vapor-liquid separator and steam injector to finishing machine.

According to Comparative Example 3, but instead of a mechanical impeller pump, a 304 austenitic steel vapor injector was used which extracted 1000 m ³ /h. The steam ejector uses 34,000,000 Kg of steam per year and costs 3 x X per year. Steam requires 1,500,000,000 L of water per year and costs X per year. Therefore, the steam ejector requires about 4 x X to operate each year.

Example 3c: Finishing machine with vapor-liquid separator and liquid ring vacuum pump.

Perform a continuous aggregation process. The effluent from the finishing machine 208 is delivered to a vent condenser 216. The vent condenser 216 includes a body reservoir 224 that is filled with a discharge line. A discharge line, sometimes referred to as a pneumatic vacuum column, is coupled to the low point of the reservoir 224.

Vacuum line 420 is coupled to a point above vent condenser 216 that is above liquid reservoir 224. Vacuum line 420 is coupled to the input of vapor-liquid separator 416. The liquid withdrawn from the low point of the vapor-liquid separator is sent to the pneumatic vacuum column as a path. The gaseous mixture above the liquid in vapor-liquid separator 416 is withdrawn via 304 austenitic steel LRVP 246C (which draws 1000 m3/h), discharged into a scrubber and vented to the atmosphere. The bypass valve 414 is coupled to the suction port and the output port of the LRVP 246C.

The respective water supply lines are coupled to a dam 218 located above the vent condenser 216 and a sprayer configuration and an upper portion of the vapor-liquid separator 416. The polymer mixture leaving LRVP 246C contained about 0.5 ppm iron, which reduced the total amount of gel produced downstream of the vacuum pump in the system to about 0.1 Kg per day, which is the rate of gel production in the process of the mechanical impeller pump of Comparative Example 3a. 20%, resulting in a long start-up time between shutdowns and cleaning. The power supplied to the liquid ring vacuum pump via the drive motor 250C is about X per year, so that the process is about 400% more efficient than the process including the steam injector in Comparative Example 3b.

Example 1 can include or use a system for continuous polyamine synthesis that can include or use a vent condenser and a vacuum pump. The vent condenser is coupled to the polymerization finisher. The vent condenser has a liquid reservoir and has a venting vent located above the liquid level of the liquid reservoir. The vacuum pump is coupled to the venting opening by a suction line. The vacuum pumps have an output port and have a rotating shaft. The gaseous mixture adjacent the venting vent is removed at a rate determined by the speed of the rotating shaft. The vacuum pump is configured to have a liquid ring seal.

Example 2 can include or optionally combine with the subject matter of Example 1 to include where the rotating shaft is coupled to an electric motor, as appropriate.

Example 3 can include or, where appropriate, the combination of the subject matter of Example 2, optionally including a speed controller coupled to the electric motor.

Example 4 can include or optionally combine with the subject matter of Example 3, including where the speed controller is coupled to a pressure sensor, a vacuum sensor, a temperature sensor, a level sensor, and a load sensor, as appropriate At least one of them.

Example 5 can include or optionally combine with the subject matter of Example 4, as the case may be, where the speed controller includes a processor coupled to the memory and the processor is configured to execute instructions stored in the memory.

Example 6 can include or optionally combine with the subject matter of any of Examples 1 through 5, as the case may be, where the vacuum pump includes a sealed fluid supply port coupled to a water supply line.

Example 7 can include or, where appropriate, the combination of the subject matter of Example 6, including where the water supply line is coupled to the cooler, as appropriate.

Example 8 can include or, as appropriate, be combined with the subject matter of any of Examples 1-7, including where the suction line includes a vapor-liquid separator, as appropriate.

Example 9 can include or optionally combine with the subject matter of Example 8, including where the vapor to liquid separator is coupled to the water supply line, as appropriate.

Example 10 can include or optionally combine with the subject matter of any of Examples 1-9, optionally including a suction port coupled to the vent condenser and further including coupling to the liquid reservoir a discharge port of the collector, and wherein the discharge port is coupled to the filter and the filter is coupled to the suction port.

Example 11 can include or optionally combine with the subject matter of Example 10 to optionally include a cooler coupled in series with the filter.

Example 12 can include or optionally combine with the subject matter of any of Examples 10 through 11 to optionally include a hydraulic pump coupled in series with the filter.

Example 13 can include or optionally combine with the subject matter of any of Examples 1 to 12, optionally including an outlet port coupled to the liquid reservoir and wherein the discharge port is coupled to an input port of the collection tank.

Example 14 can include or optionally combine with the subject matter of Example 13, including, where appropriate, the collection trough including a dam and an exit port, and wherein the input port and the exit port are disposed on opposite sides of the barrage.

Example 15 can include or optionally combine with the subject matter of any of Examples 1-14, including where the output port is coupled to an atmospheric vent, as appropriate.

Example 16 can include or optionally combine with the subject matter of Example 15 to include where the atmospheric vent includes a stacked scrubber.

Example 17 can include or optionally combine with the subject matter of any of Examples 1-16, optionally including a bypass valve coupled in series with the vacuum pump.

Example 18 can include or optionally combine with the subject matter of Example 17, including, where appropriate, the gaseous mixture being removed at a rate determined by the flow rate of the fluid through the bypass valve.

Example 19 can include or use a method of operating a polymerization finisher stage of a continuous polyamine synthesis system that can include or use a gaseous mixture in the upper region of the reservoir and withdraw the gaseous mixture from the upper region using a vacuum. A gaseous mixture is produced in an upper region of the reservoir coupled to the finishing machine. The reservoir has a liquid level in the area of the lower portion of the reservoir. The gaseous mixture is withdrawn from the upper region using a vacuum, wherein the removal rate corresponds to the speed of the rotating shaft of the liquid ring vacuum pump.

Example 20 can include or optionally combine with the subject matter of Example 19 to optionally operate the vacuum pump using an electric motor.

Example 21 may include or optionally combine with the subject matter of Example 19 to optionally adjust the speed using a controller.

Example 22 may include or, as appropriate, be combined with the subject matter of Example 21, as the case may be, where it is contemplated that adjusting the speed includes performing a algorithm using a processor.

Example 23 can include or optionally combine with the subject matter of Example 22, as the case may be, where it is contemplated that performing the algorithm includes accepting a sensor signal corresponding to at least one of pressure, vacuum, temperature, level, and load.

Example 24 can include or optionally combine with the subject matter of Example 19, including optionally wherein discharging the gaseous mixture includes providing water to a sealed fluid port of the vacuum pump.

Example 25 can include or optionally combine with the subject matter of Example 24, including optionally including providing water therein including cooling the water.

Example 26 can include or optionally combine with the subject matter of any of Examples 19-25, including optionally removing vapor from the vapor-liquid separator that is self-coupled to the upper region.

Example 27 can include or optionally combine with the subject matter of Example 26 to optionally supply water to the vapor-liquid separator.

Example 28 can include or optionally combine with the subject matter of any of Examples 19-27, including optionally removing liquid from the lower region, filtering the liquid, and returning the liquid to the upper region.

Example 29 can include or optionally combine with the subject matter of Example 28, optionally including cooling the liquid.

Example 30 can include or optionally combine with the subject matter of any of Examples 19-29, optionally including removing liquid from the lower region and delivering the liquid to the collection tank.

Example 31 can include or optionally combine with the subject matter of Example 30, as the case may include The liquid is discharged from the dam and discharge port of the collection tank.

Example 32 can include or optionally combine with the subject matter of any of Examples 19-31, including optionally wherein extracting the gaseous mixture includes discharging the output of the vacuum pump to the atmosphere.

Example 33 can include or optionally combine with the subject matter of any of Examples 19 to 32, optionally including bypassing the vacuum pump with a valve.

Each of these non-limiting examples may exist independently or in various permutations or in combination with one or more other examples.

The above [embodiment] includes a reference to the accompanying drawings, which form part of the [embodiment] with the accompanying drawings. The drawings show specific examples in which the invention may be practiced. Such examples may include elements in addition to those described or described. However, the inventors of the present invention also cover examples of providing only those elements shown or described. In addition, the inventors of the present invention also cover the use of such a specific example (or one or more aspects thereof) or other examples (or one or more aspects thereof) shown or described herein. Examples of any combination or arrangement of the elements shown or described (or one or more aspects thereof).

In the event that this document is inconsistent with the usage of any of the documents so incorporated by reference, the usage in this document is primarily.

In this document, as commonly used in the patent literature, the term "a" is used to include one or more, and "at least one" or "one or more". Any other instance or usage of the species). In this document, the term "or" is used to mean non-exclusive or such that "A or B" includes "A, not B", "B, not A" and "A and B". In this document, the terms "including" and "in which" are used as the plain English synonym for the individual terms "comprising" and "wherein". In addition, in the following claims, the terms "including" and "comprising" are open, that is, systems, devices, articles, and compositions that include elements other than those listed after such terms in the technical solutions. Formula or system Cheng is still considered to belong to the scope of his technical solutions. In addition, in the following claims, the terms "first", "second", "third", etc. are used only as labels, and do not impose numerical requirements on their objects.

Examples of methods described herein can be implemented at least in part for a machine or computer. Some examples may include a computer readable medium or machine readable medium encoded with instructions operable to configure an electronic device to perform the methods as described in the above examples. Implementations of such methods may include code, such as microcode, combined language code, high level language code, or the like. Such code may include computer readable instructions for performing various methods. The code can form part of a computer program product. Moreover, in an example, such as during execution or at other times, the code is tactilely stored on one or more volatile, non-transitory or non-volatile, tactile, computer readable media. Examples of such tangible computer readable media may include, but are not limited to, hard disks, removable disks, removable optical disks (eg, compact disks and digital video disks), cassette tapes, memory cards, or Stick, random access memory (RAM), read only memory (ROM) and the like.

The above description is intended to be illustrative, and not restrictive. For example, the examples described above (or one or more aspects thereof) can be used in combination with one another. Other examples may be used by those of ordinary skill in the art when reviewing the above description. Providing [Abstract] allows the reader to quickly determine the nature of the technical invention. The Abstract is submitted with an understanding of the scope or meaning of the scope of the patent application. In addition, in the above embodiments, various features may be grouped together to simplify the present invention. This should not be construed as requiring that the disclosed features not claimed are essential to any technical solution. On the contrary, the subject matter of the invention may be in all the features of the specific disclosed examples. Therefore, the scope of the following patent application is hereby incorporated by reference in its entirety as the same as the same as the same as the same, and the examples may be intended to be combined with each other in different combinations or arrangements. The scope of the subject matter of the present invention should be determined by reference to the scope of the appended claims and the scope of the claims.

8‧‧‧ pipeline

10‧‧‧System

12‧‧‧Reservoir

14‧‧‧Evaporator

16‧‧‧ pipeline

18‧‧‧Reactor

22‧‧‧ pipeline

24‧‧‧Condenser

26‧‧‧ pipeline

28‧‧‧ pipeline

30‧‧‧Flasher

32‧‧‧ pipeline

34‧‧‧ pipeline

208‧‧‧ Finishing machine

Claims (20)

A method of operating a polymerization finisher stage of a continuous polyamine synthesis system, the method comprising: generating a gaseous mixture in an upper region of a reservoir coupled to the finisher, the reservoir having the reservoir The liquid level in the lower region of the device; and the gaseous mixture is withdrawn from the upper region using a vacuum, wherein the removal rate corresponds to the velocity of the rotating shaft of the liquid ring vacuum pump. The method of claim 1, further comprising operating the vacuum pump using a motor. The method of claim 1, further comprising adjusting the speed using a controller. The method of claim 3, wherein adjusting the speed comprises performing an algorithm using a processor. The method of claim 4, wherein performing the algorithm comprises accepting a sensor signal corresponding to at least one of pressure, vacuum, temperature, level, and load. The method of any one of claims 1 to 5, wherein discharging the gaseous mixture comprises providing water to a sealed fluid port of the vacuum pump. The method of claim 6, wherein providing the water comprises cooling the water. The method of any one of claims 1 to 7, wherein extracting the gaseous mixture comprises vapor-liquid separator auto-coupling to the upper region to remove vapor. The method of claim 8 further comprising supplying water to the vapor-liquid separator. The method of any one of claims 1 to 9, further comprising removing liquid from the lower region, filtering the liquid, and returning the liquid to the upper region. The method of claim 10, further comprising cooling the liquid. The method of any one of claims 1 to 11, further comprising removing liquid from the lower region and delivering the liquid to the collection tank. The method of claim 12, further comprising using the collection tank for dam and discharge The mouth discharges the liquid. The method of any one of claims 1 to 13, wherein extracting the gaseous mixture comprises discharging the output of the vacuum pump to the atmosphere. The method of any one of claims 1 to 14, further comprising bypassing the vacuum pump with a valve. A system for continuous polyamine synthesis, the system comprising: a vent condenser coupled to a polymerization finisher, the vent condenser having a liquid reservoir and having a venting above the liquid level of the liquid reservoir a discharge port; and a vacuum pump coupled to the venting opening by a suction line, the vacuum pump having an output port and having a rotating shaft, and wherein the gaseous mixture adjacent to the venting opening is removed at a rate determined by the speed of the rotating shaft The vacuum pump is configured to have a liquid ring seal. The system of claim 16, further comprising a suction port coupled to the vent condenser and further comprising a discharge port coupled to the liquid reservoir, and wherein the discharge port is coupled to the filter, and the filtering The device is coupled to the suction port. The system of any one of claims 16 to 17, further comprising a discharge port coupled to the liquid reservoir, and wherein the discharge port is coupled to the input port of the collection tank. The system of claim 18, wherein the collection trough comprises a dam and an exit port, and wherein the input port and the exit port are disposed on opposite sides of the barrage. The system of any one of claims 16 to 19, wherein the output port is coupled to an atmospheric vent.